CN101462034A - Method for preparing nanoparticles - Google Patents
Method for preparing nanoparticles Download PDFInfo
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- CN101462034A CN101462034A CNA2007100326063A CN200710032606A CN101462034A CN 101462034 A CN101462034 A CN 101462034A CN A2007100326063 A CNA2007100326063 A CN A2007100326063A CN 200710032606 A CN200710032606 A CN 200710032606A CN 101462034 A CN101462034 A CN 101462034A
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Abstract
The invention discloses a method for preparing a superfine self-reaction micro-emulsion nanometer particle. The method takes an aqueous solution of a soluble salt as a raw material, a surfactant as a dispersing agent, an oxidizing agent or a reducing agent and a stabilizing agent and alkane or other organic matters as a solvent. The method is characterized in that the aqueous solution of the soluble salt is added to an alkane oil phase which contains the surfactant and the solvent to form a water-in-oil micro-emulsion system, and the soluble salt reacts with the surfactant to generate products. The preparation method is a method by which nanometer particles of various materials can be prepared, so the method has wide applicability; and the prepared nanometer particle material is widely applied in fields such as electronic industry, chemical industry and the like.
Description
Technical field:
The present invention relates to a kind of preparation of nanomaterials, particularly a kind of preparation method of autoreaction emulsion nanometer particle.
Background technology:
Nano material, particularly nano particle is the material of a kind of brand new of growing up the eighties in 20th century, because its significant skin effect, quantum size effect and macro quanta tunnel effect etc., nano material shows unusual electricity, magnetics, calorifics, mechanics, optics and chemical characteristic, has showed application prospects in chemical industry, microelectronics, environment, the energy, military affairs, medicine and other fields.
The technology of preparing of nano particle is the basis that nano material is used, and preparation technology and process control have significant effects to the structure and the performance of nano particle.Because microemulsion method can be controlled the advantage of nanometer particle size and surface topography, it has been widely used among the preparation technology of nano particle.The thermodynamically stable system that microemulsion is made up of water, surfactant, cosurfactant and oil phase, wherein water forms small pond among being dispersed in oil phase by surfactant and cosurfactant, meet in the pond of this small pond and another kind of reactant, counterdiffusion of reactant phase and reaction generate product.Wherein, surfactant and cosurfactant only play peptizaiton and stabilization, because reaction rear surface activating agent and oil phase reclaim difficulty, and in preparation process, need to prepare the microemulsion of various reactants, therefore conventional method has a large amount of wastes of surfactant and solvent, the preparation section complexity, shortcoming such as consuming time has influenced the large-scale application of these class methods.
Summary of the invention:
Technical problem to be solved by this invention overcomes existing deficiency among the present preparation technology exactly, a kind of method for preparing nano particle is provided, this preparation method is to be dispersant, stabilizing agent and oxidation (or reduction) agent with the surfactant, the aqueous solution of soluble-salt is scattered in the water in oil microemulsion system of formation in the solvent alkanes oil phase, solubility salt and surfactant reaction then generates product, expect that from former product one step makes, preparation is simple, quick, and can save surfactant and solvent in a large number.
For solving the problems of the technologies described above, the present invention has adopted following technical scheme: the present invention is a raw material with the aqueous solution of soluble-salt, with the surfactant is dispersant, oxidation or reducing agent and stabilizing agent, with alkane or other organic matters is solvent, at first, the aqueous solution of soluble-salt join contain surfactant and organic solvent, and finely dispersed oil phase in, by stirring or ultrasonic dispersing mode forms water-in-oil microemulsion; Secondly, continue to stir or ultrasonic dispersion, finish, generate product up to the oxidation or the reduction reaction of soluble-salt and surfactant; At last, reaction is finished postprecipitation and is filtered, and water and absolute ethyl alcohol fully wash, oven dry.
The product that the present invention produced is metal simple-substance or alloy.As gold, silver, platinum, iron, cobalt, nickel, violent, titanium, vanadium or their alloy.Perhaps be the oxide or the salt of metal.Oxide as iron, cobalt, nickel, violent, titanium, vanadium.Being shaped as of these products is spherical, bar-shaped, hollow ball, tubulose, sheet, wire shape, and its particle degree at least on a dimension less than 100 nanometers.
Soluble-salt described in the technique scheme is: following salt a kind of: 1, permanganate, as potassium permanganate, sodium permanganate; 2, nitrate is as manganese nitrate, ferric nitrate, cobalt nitrate; 3, sulfate, manganese sulfate, ferric sulfate, ferrous sulfate; 4, chloride is as manganese chloride; 5, alum salts is as sodium vanadate, alum acid potassium; 6, tungstates is as sodium tungstate, potassium tungstate.
Organic solvent described in the technique scheme selects for use one or more to contain the alkane of 6～22 carbon.
The aqueous solution of soluble-salt is scattered in the solvent in the technique scheme, also reaction generates in the product process with it, select for use at least a surfactant to adjust the shape of the forming process of emulsion, participation preparation feedback, control product, described surfactant is: if anionic surfactant adopts: the succinate sulfonate; Or alkyl sulfonate; Or alkylbenzene sulfonate.If cationic surface active agent adopts: alkyl trimethyl ammonium salt; Or two alkyl dimethyl ammonium salts; Or benzyl dimethyl ammonium salt; If not ionic surfactant, especially polyethenoxy ether class R-(OCH
2CH
2)
n～OH, wherein R is the alkyl of 2～18 carbon, n is 2～8.Perhaps select alcohols R-CH
2-OH, wherein R is for containing the alkyl of 2-18 carbon.
In the technique scheme, the molar ratio of water and surfactant is between 5～100.
The present invention is different from common chemical method and microemulsion method, and it is that the aqueous solution with soluble-salt is formed water in oil microemulsion system by surfactant-dispersed in solvent alkanes oil phase, and solubility salt and surfactant reaction then generates product.The present invention is dispersant, stabilizing agent and oxidation (or reduction) agent with the surfactant, the aqueous solution of soluble-salt is scattered in the water in oil microemulsion system of formation in the solvent hydro carbons oil phase, then the solubility salt is generated product by the surfactant reaction, expect that from former product one step makes, preparation is simple, quick, and can save surfactant and solvent in a large number.The purpose of this invention is to provide a kind of method for preparing nano material, enable to control the method for nano material shape, size and surface topography.The present invention studies the commercial Application aspect from the preparation method and has important theory and realistic meaning.
The specific embodiment:
The present invention is dispersant, stabilizing agent and oxidation (or reduction) agent with the surfactant, the aqueous solution of soluble-salt is scattered in the water in oil microemulsion system of formation in the solvent hydro carbons oil phase, then the solubility salt is generated product by the surfactant reaction, and detailed process is as follows:
At first, the aqueous solution of soluble-salt join contain surfactant and organic solvent, and finely dispersed oil phase in, by stirring or ultrasonic dispersing mode forms water-in-oil microemulsion.
Here said soluble-salt is: following salt a kind of: 1, permanganate, as potassium permanganate, sodium permanganate; 2, nitrate is as manganese nitrate, ferric nitrate, cobalt nitrate; 3, sulfate, manganese sulfate, ferric sulfate, ferrous sulfate; 4, chloride is as manganese chloride; 5, alum salts is as sodium vanadate, alum acid potassium; 6, tungstates is as sodium tungstate, potassium tungstate.
Its organic solvent that adopts selects for use one or more to contain the alkane of 6～22 carbon.The surfactant that is adopted comprises following four kinds:
One, anionic surfactant, preferred:
(a) succinate sulfonate
Wherein R and R ' are the alkyl of 2～18 carbon, preferentially are sulfosuccinic acid methyl-isobutyl methyl esters sodium;
(b) alkyl sulfonate R-SO
3Na, wherein R is the alkyl of 2～18 carbon, preferentially is dodecyl semi-annular jade pendant acid sodium;
(c) benzene sulfonate R-(C
6H
6)-SO
3Na, wherein R is the alkyl of 2～18 carbon, preferentially is detergent alkylate semi-annular jade pendant acid sodium;
Two, cationic surface active agent, preferred:
I. alkyl trimethyl ammonium salt or two alkyl dimethyl ammonium salt
Wherein, R and R ' are for containing the alkyl of 1～18 carbon, and X is Br or Cl, preferentially is cetyl trimethyl ammonia bromide and OTAC.
Ii. benzyl dimethyl ammonium salt
Wherein, R is the alkyl that contains 1～18 carbon, and X is Br or Cl, such as the octadecyl alkyl dimethyl ammonium chloride.
Three, nonionic surface active agent, preferred:
Polyethenoxy ether class R-(OCH
2CH
2)
n-OH, wherein R is the alkyl of 2～18 carbon, n is 2～8;
Four, alcohols R-CH
2-OH, wherein R is for containing the alkyl of 2-18 carbon.
In addition, in preparation process, the molar ratio of water and surfactant is between 5～100.
Secondly, after finishing above-mentioned technology, continue to stir or ultrasonic dispersion, finish, generate product up to the oxidation or the reduction reaction of soluble-salt and surfactant;
At last, reaction is finished postprecipitation and is filtered, and water and absolute ethyl alcohol fully wash, oven dry.But according to different raw materials, last resultant product is also different, and it can be divided into: 1, metal simple-substance or alloy.As gold, silver, platinum, iron, cobalt, nickel, violent, titanium, vanadium or their alloy.2, the oxide of metal or salt.Oxide as iron, cobalt, nickel, violent, titanium, vanadium.Shapes such as that the shape of these products is generally is spherical, bar-shaped, hollow ball, tubulose, sheet, wire, and its particle degree at least on a dimension less than 100 nanometers.
Embodiment 1: room temperature, to put into 60ml normal octane solvent as the 17.324g cetyl trimethyl ammonia bromide (CTAB) of cationic surface active agent and 13.858g n-butanol earlier stirs, add the potassium permanganate solution that 35mL concentration is 0.1mol/L while stirring, after all adding, continue to stir 4 hours.Carry out suction filtration then, water and absolute ethyl alcohol filter respectively 5 times, obtain the brown filter cake, and oven dry promptly obtains the manganese oxide nano particle.
Embodiment 2: room temperature, to put into 60ml isooctane solvent as the 5.956g cetyl trimethyl ammonia bromide (CTAB) of cationic surface active agent and 4.764g isobutanol earlier stirs, add the potassium permanganate solution that 10mL concentration is 0.15mol/L while stirring, after all adding, continue to stir 4 hours.Carry out suction filtration then, water and absolute ethyl alcohol filter respectively 5 times, obtain the brown filter cake, and oven dry promptly obtains the manganese oxide nano particle.
Claims (9)
1, a kind of nanometer particle process method, its aqueous solution with soluble-salt is raw material, is dispersant, oxidation or reducing agent and stabilizing agent with the surfactant, is solvent with alkane or other organic matters, it is characterized in that:
At first, the aqueous solution of soluble-salt join contain surfactant and organic solvent, and finely dispersed oil phase in, by stirring or ultrasonic dispersing mode forms water-in-oil microemulsion;
Secondly, continue to stir or ultrasonic dispersion, finish, generate product up to the oxidation or the reduction reaction of soluble-salt and surfactant;
At last, reaction is finished postprecipitation and is filtered, and water and absolute ethyl alcohol fully wash, oven dry.
2, a kind of nanometer particle process method according to claim 1, it is characterized in that: the product of being produced is metal simple-substance or alloy.
3, a kind of nanometer particle process method according to claim 1 is characterized in that: the product of being produced is the oxide or the salt of metal.
4, a kind of nanometer particle process method according to claim 1 is characterized in that: the product of being produced is spherical, bar-shaped, hollow ball, tubulose, sheet, wire shape.
5, a kind of nanometer particle process method according to claim 1 is characterized in that: the particle degree of the product of being produced at least on a dimension less than 100 nanometers.
6, a kind of nanometer particle process method according to claim 1, it is characterized in that: described soluble-salt is: following salt a kind of: permanganate, nitrate, sulfate, chloride, alum salts, alum acid potassium, tungstates.
7, a kind of nanometer particle process method according to claim 1 is characterized in that: described organic solvent selects for use one or more to contain the alkane of 6～22 carbon.
8, a kind of nanometer particle process method according to claim 1, it is characterized in that: the aqueous solution of soluble-salt is scattered in the solvent, also reaction generates in the product process with it, select for use at least a surfactant to adjust the shape of the forming process of emulsion, participation preparation feedback, control product, described surfactant is:
One, anionic surfactant, adopt:
(a) succinate sulfonate
Wherein R and R ' are the alkyl of 2～18 carbon;
(b) alkyl sulfonate R-SO
3Na, wherein R is the alkyl of 2～18 carbon;
(c) alkylbenzene sulfonate R-(C
6H
6)-SO
3Na, wherein R is the alkyl of 2～18 carbon; Two, cationic surface active agent, adopt:
(d) alkyl trimethyl ammonium salt or two alkyl dimethyl ammonium salt
Wherein, R and R ' are for containing the alkyl of 1～18 carbon, and X is Br or Cl;
(e) benzyl dimethyl ammonium salt
Wherein, R is the alkyl that contains 1～18 carbon, and X is Br or Cl;
Three, nonionic surface active agent, adopt:
Polyethenoxy ether class R-(OCH
2CH
2)
n-OH, wherein R is the alkyl of 2～18 carbon, n is 2～8;
Four, alcohols R-CH
2-OH, wherein R is for containing the alkyl of 2-18 carbon.
9, a kind of nanometer particle process method according to claim 1, it is characterized in that: the molar ratio of water and surfactant is between 5～100.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100326063A CN101462034A (en) | 2007-12-18 | 2007-12-18 | Method for preparing nanoparticles |
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|---|---|---|---|
| CNA2007100326063A CN101462034A (en) | 2007-12-18 | 2007-12-18 | Method for preparing nanoparticles |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102064326A (en) * | 2010-12-16 | 2011-05-18 | 东莞新能源电子科技有限公司 | Dispersing agent for positive and negative electrode materials of lithium ion battery |
| CN108288712A (en) * | 2017-12-21 | 2018-07-17 | 浙江天能能源科技股份有限公司 | A kind of lithium ion battery negative material Fe2O3Preparation method |
| WO2019037021A1 (en) * | 2017-08-21 | 2019-02-28 | 中国科学技术大学 | Photochromic nanomaterial capable of blocking ultraviolet rays and preparation method and use thereof |
| CN109421485A (en) * | 2017-08-21 | 2019-03-05 | 中国科学技术大学 | Can ultraviolet blocking-up the preparation method of photochromic vehicle window and products thereof and application |
| CN109530717A (en) * | 2018-12-03 | 2019-03-29 | 安徽工业大学 | The method of microemulsion method controlledly synthesis Ag metal nano material in original position from Ag-containing solution |
| CN106660128B (en) * | 2014-05-19 | 2019-11-05 | 同和电子科技有限公司 | Silver particles dispersion liquid |
| CN112779550A (en) * | 2021-01-11 | 2021-05-11 | 中山大学 | Three-dimensional micron tubular hydrogen evolution reaction electrocatalyst and preparation method thereof |
-
2007
- 2007-12-18 CN CNA2007100326063A patent/CN101462034A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102064326A (en) * | 2010-12-16 | 2011-05-18 | 东莞新能源电子科技有限公司 | Dispersing agent for positive and negative electrode materials of lithium ion battery |
| CN106660128B (en) * | 2014-05-19 | 2019-11-05 | 同和电子科技有限公司 | Silver particles dispersion liquid |
| WO2019037021A1 (en) * | 2017-08-21 | 2019-02-28 | 中国科学技术大学 | Photochromic nanomaterial capable of blocking ultraviolet rays and preparation method and use thereof |
| CN109421485A (en) * | 2017-08-21 | 2019-03-05 | 中国科学技术大学 | Can ultraviolet blocking-up the preparation method of photochromic vehicle window and products thereof and application |
| CN109424306A (en) * | 2017-08-21 | 2019-03-05 | 中国科学技术大学 | Can ultraviolet blocking-up photochromic building window preparation method and application |
| JP2019536824A (en) * | 2017-08-21 | 2019-12-19 | 中国科学技▲術▼大学Ｕｎｉｖｅｒｓｉｔｙ Ｏｆ Ｓｃｉｅｎｃｅ Ａｎｄ Ｔｅｃｈｎｏｌｏｇｙ Ｏｆ Ｃｈｉｎａ | Photochromic nanomaterial capable of blocking ultraviolet rays, method for producing the same and use thereof |
| CN109424306B (en) * | 2017-08-21 | 2020-08-25 | 中国科学技术大学 | Preparation method and application of photochromic building window capable of blocking ultraviolet rays |
| US11008220B2 (en) | 2017-08-21 | 2021-05-18 | University Of Science And Technology Of China | Photochromic nanomaterial capable of blocking ultraviolet rays, production method and use thereof |
| CN108288712A (en) * | 2017-12-21 | 2018-07-17 | 浙江天能能源科技股份有限公司 | A kind of lithium ion battery negative material Fe2O3Preparation method |
| CN109530717A (en) * | 2018-12-03 | 2019-03-29 | 安徽工业大学 | The method of microemulsion method controlledly synthesis Ag metal nano material in original position from Ag-containing solution |
| CN112779550A (en) * | 2021-01-11 | 2021-05-11 | 中山大学 | Three-dimensional micron tubular hydrogen evolution reaction electrocatalyst and preparation method thereof |
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Open date: 20090624 |